Sodium Hydroxide → HCID 22643234, 화합물

HRID 2414755노트

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HRID 2414755 반응식
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([NH:12]C(=O)C)[CH:10]=2)[N:5]=[C:4]([C:16]2[CH:21]=[CH:20][C:19]([CH:22]3[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]3)=[CH:18][CH:17]=2)[CH:3]=1.[OH-].[Na+]>Cl>[CH:22]1([C:19]2[CH:18]=[CH:17][C:16]([C:4]3[CH:3]=[C:2]([NH2:1])[C:11]4[C:6](=[CH:7][CH:8]=[C:9]([NH2:12])[CH:10]=4)[N:5]=3)=[CH:21][CH:20]=2)[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27]1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 22643183HCID 22643183, 화합물

생성물 1

HCID 22643234HCID 22643234, 화합물수율 87.5%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

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온도
95 °C

실험 절차

N-[4-Amino-2-(4-cyclohexylphenyl)-quinolin-6-yl]-acetamide (22 g) was placed in a 1 L flask to which 500 mL of 6 N HCl was added and the mixture heated with stirring to 95° C. for 18 hrs. After this time, the solution was cooled in ice and was then cautiously neutralized with concentrated NaOH solution, followed by adjustment to pH 9.5. The solution was then poured into a 2 L separatory funnel and extracted with ethyl acetate. The organic layer was then dried over Na2SO4, filtered and concentrated to give 17 g of the desired product. Repeated crystallization using methanol, methylene chloride and hexane provided 9.0 g (41%) of the pure title compound.

후처리

  1. additionwas added
  2. temperaturethe mixture heated
  3. temperatureAfter this time, the solution was cooled in ice
  4. additionThe solution was then poured into a 2 L separatory funnel
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic layer was then dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-46a1bce4257349b38391b9a69d214e9d
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06815447B2

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